JP2013147678A - 金属銅焼結膜の製造方法 - Google Patents
金属銅焼結膜の製造方法 Download PDFInfo
- Publication number
- JP2013147678A JP2013147678A JP2012006955A JP2012006955A JP2013147678A JP 2013147678 A JP2013147678 A JP 2013147678A JP 2012006955 A JP2012006955 A JP 2012006955A JP 2012006955 A JP2012006955 A JP 2012006955A JP 2013147678 A JP2013147678 A JP 2013147678A
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- Prior art keywords
- film
- acid
- metal copper
- metallic copper
- gelatin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- 239000010949 copper Substances 0.000 title claims abstract description 150
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 149
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 149
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 14
- 239000002245 particle Substances 0.000 claims abstract description 82
- 108010010803 Gelatin Proteins 0.000 claims abstract description 63
- 239000008273 gelatin Substances 0.000 claims abstract description 63
- 229920000159 gelatin Polymers 0.000 claims abstract description 63
- 235000019322 gelatine Nutrition 0.000 claims abstract description 63
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 63
- 229920000642 polymer Polymers 0.000 claims abstract description 48
- 239000002270 dispersing agent Substances 0.000 claims abstract description 41
- 238000000034 method Methods 0.000 claims abstract description 38
- 239000003960 organic solvent Substances 0.000 claims abstract description 23
- 229910052751 metal Inorganic materials 0.000 claims description 91
- 239000002184 metal Substances 0.000 claims description 91
- 239000002253 acid Substances 0.000 claims description 60
- -1 glycol ethers Chemical class 0.000 claims description 46
- 150000001412 amines Chemical class 0.000 claims description 38
- 239000006185 dispersion Substances 0.000 claims description 27
- 239000000463 material Substances 0.000 claims description 20
- 238000000576 coating method Methods 0.000 claims description 15
- 239000011248 coating agent Substances 0.000 claims description 13
- LYCAIKOWRPUZTN-UHFFFAOYSA-N ethylene glycol Natural products OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 9
- 230000008569 process Effects 0.000 claims description 5
- 150000001298 alcohols Chemical class 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 4
- 150000002576 ketones Chemical class 0.000 claims description 4
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 description 27
- 229960004643 cupric oxide Drugs 0.000 description 25
- 239000005751 Copper oxide Substances 0.000 description 23
- 239000008139 complexing agent Substances 0.000 description 23
- 229910000431 copper oxide Inorganic materials 0.000 description 23
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 18
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 18
- 229910052717 sulfur Inorganic materials 0.000 description 18
- 239000011593 sulfur Substances 0.000 description 18
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- 239000002585 base Substances 0.000 description 17
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 6
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 6
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- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
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- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 4
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 description 4
- 229910052783 alkali metal Inorganic materials 0.000 description 4
- 125000000217 alkyl group Chemical group 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- HQABUPZFAYXKJW-UHFFFAOYSA-N butan-1-amine Chemical compound CCCCN HQABUPZFAYXKJW-UHFFFAOYSA-N 0.000 description 4
- 239000000084 colloidal system Substances 0.000 description 4
- SWXVUIWOUIDPGS-UHFFFAOYSA-N diacetone alcohol Chemical compound CC(=O)CC(C)(C)O SWXVUIWOUIDPGS-UHFFFAOYSA-N 0.000 description 4
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 4
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 description 4
- 229910001882 dioxygen Inorganic materials 0.000 description 4
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 4
- 229910052734 helium Inorganic materials 0.000 description 4
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Images
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- Parts Printed On Printed Circuit Boards (AREA)
- Powder Metallurgy (AREA)
- Manufacturing Of Printed Wiring (AREA)
- Non-Insulated Conductors (AREA)
- Manufacturing Of Electric Cables (AREA)
Abstract
【解決手段】 ゼラチンを粒子表面に有する金属銅粒子、高分子分散剤及び有機溶媒を含む分散液を用いて基材の表面に金属銅含有膜を形成し、次いで、その金属銅含有膜の全領域又は一部領域にプラズマ処理する工程を含むことにより、低温度でも大量に焼結処理が可能であり、製造した金属銅焼結膜の抵抗値は十分低く、電極、配線パターン、塗膜等に用いることができる。
【選択図】図1
Description
本発明で製造した金属銅焼結膜は、電極、配線パターン又は塗膜等に用いることができる。具体的には、金属銅焼結膜の体積抵抗値は20μΩ・cm以下のものが得られ、また、膜厚の薄い焼結膜とすることができることから、プリンタブルエレクトロニクス分野でのプリント配線基板等の微細電極及び回路配線パターンに特に有用である。
(アミン価の測定方法)
ゼラチン又は高分子分散剤5g、ブロモクレゾールグリーンエタノール溶液数滴を300mLのエタノールと純水の混合溶媒に溶解させ、ファクター(補正係数)を算出した0.1M HClエタノール溶液を添加し、ブロモクレゾールグリーン指示薬の黄色が30秒続いた時の0.1M HClエタノール溶液の滴定量からアミン価を算出する。
(酸価の測定方法)
ゼラチン又は高分子分散剤5g、フェノールフタレイン液数滴を300mLの純水に溶解させ、ファクター(補正係数)を算出した0.1M KOHエタノール溶液を添加する。フェノールフタレイン指示薬の薄紅色が30秒続いた時の0.1M KOHエタノール溶液の滴定量から酸価を算出する。
(1)窒素がドナー原子である錯化剤としては、(a)アミン類(例えば、ブチルアミン、エチルアミン、プロピルアミン、エチレンジアミン等の1級アミン類、ジブチルアミン、ジエチルアミン、ジプロピルアミン、及び、ピペリジン、ピロリジン等のイミン類等の2級アミン類、トリブチルアミン、トリエチルアミン、トリプロピルアミン等の3級アミン類、ジエチレントリアミン、トリエチレンテトラミンの1分子内に1〜3級アミンを2種以上有するもの等)、(b)窒素含有複素環式化合物(例えば、イミダゾール、ピリジン、ビピリジン等)、(c)ニトリル類(例えば、アセトニトリル、ベンゾニトリル等)及びシアン化合物、(d)アンモニア及びアンモニウム化合物(例えば、塩化アンモニウム、硫酸アンモニウム等)、(e)オキシム類等が挙げられる。
(2)酸素がドナー原子である錯化剤としては、(a)カルボン酸類(例えば、クエン酸、リンゴ酸、酒石酸、乳酸等のオキシカルボン酸類、酢酸、ギ酸等のモノカルボン酸類、シュウ酸、マロン酸等のジカルボン酸類、安息香酸等の芳香族カルボン酸類等)、(b)ケトン類(例えば、アセトン等のモノケトン類、アセチルアセトン、ベンゾイルアセトン等のジケトン類等)、(c)アルデヒド類、(d)アルコール類(1価アルコール類、グリコール類、グリセリン類等)、(e)キノン類、(f)エーテル類、(g)リン酸(正リン酸)及びリン酸系化合物(例えば、ヘキサメタリン酸、ピロリン酸、亜リン酸、次亜リン酸等)、(h)スルホン酸又はスルホン酸系化合物等が挙げられる。
(3)硫黄がドナー原子である錯化剤としては、(a)脂肪族チオール類(例えば、メチルメルカプタン、エチルメルカプタン、プロピルメルカプタン、イソプロピルメルカプタン、n−ブチルメルカプタン、アリルメルカプタン、ジメチルメルカプタン等)、(b)脂環式チオール類(シクロヘキシルチオール等)、(c)芳香族チオール類(チオフェノール等)、(d)チオケトン類、(e)チオエーテル類、(f)ポリチオール類、(g)チオ炭酸類(トリチオ炭酸類)、(h)硫黄含有複素環式化合物(例えば、ジチオール、チオフェン、チオピラン等)、(i)チオシアナート類及びイソチオシアナート類、(j)無機硫黄化合物(例えば、硫化ナトリウム、硫化カリウム、硫化水素等)等が挙げられる。
(4)2種以上のドナー原子を有する錯化剤としては、(a)アミノ酸類(ドナー原子が窒素及び酸素:例えば、グリシン、アラニン等の中性アミノ酸類、ヒスチジン、アルギニン等の塩基性アミノ酸類、アスパラギン酸、グルタミン酸等の酸性アミノ酸類)、(b)アミノポリカルボン酸類(ドナー原子が窒素及び酸素:例えば、エチレンジアミンテトラ酢酸(EDTA)、ニトリロトリ酢酸(NTA)、イミノジ酢酸(IDA)、エチレンジアミンジ酢酸(EDDA)、エチレングリコールジエチルエーテルジアミンテトラ酢酸(GEDA)等)、(c)アルカノールアミン類(ドナー原子が窒素及び酸素:例えば、エタノールアミン、ジエタノールアミン、トリエタノールアミン等)、(d)ニトロソ化合物及びニトロシル化合物(ドナー原子が窒素及び酸素)、(e)メルカプトカルボン酸類(ドナーが硫黄及び酸素:例えば、メルカプトプロピオン酸、メルカプト酢酸、チオジプロピオン酸、メルカプトコハク酸、ジメルカプトコハク酸、チオ酢酸、チオジグリコール酸等)、(f)チオグリコール類(ドナーが硫黄及び酸素:例えば、メルカプトエタノール、チオジエチレングリコール等)、(g)チオン酸類(ドナーが硫黄及び酸素)、(h)チオ炭酸類(ドナー原子が硫黄及び酸素:例えば、モノチオ炭酸、ジチオ炭酸、チオン炭酸)、(i)アミノチオール類(ドナーが硫黄及び窒素:アミノエチルメルカプタン、チオジエチルアミン等)、(j)チオアミド類(ドナー原子が硫黄及び窒素:例えば、チオホルムアミド等)、(k)チオ尿素類(ドナー原子が硫黄及び窒素)、(l)チアゾール類(ドナー原子が硫黄及び窒素:例えばチアゾール、ベンゾチアゾール等)、(m)含硫黄アミノ酸類(ドナーが硫黄、窒素及び酸素:システイン、メチオニン等)等が挙げられる。
(5)上記の化合物の塩や誘導体としては、例えば、クエン酸トリナトリウム、酒石酸ナトリウム・カリウム、次亜リン酸ナトリウム、エチレンジアミンテトラ酢酸ジナトリウム等のそれらのアルカリ金属塩や、カルボン酸、リン酸、スルホン酸等のエステル等が挙げられる。
このような錯化剤のうち、少なくとも1種を用いることができる。錯化剤の使用量は錯化剤の種類により最適量が異なるため、その種類に応じて適宜設定する。錯化剤の使用量を少なくすると、金属銅微粒子の一次粒子を小さくすることができ、使用量を多くすると、一次粒子を大きくすることができる。
工業用酸化第二銅(エヌシーテック社製N−120)24g、保護コロイドとしてゼラチン(アミン価23、酸価29、アミン価−酸価=−6)2.8gを150ミリリットルの純水に添加、混合し、15%のアンモニア水を用いて混合液のpHを11に調整した後、20分かけて室温から90℃まで昇温した。昇温後、撹拌しながら、錯化剤として1%の3−メルカプトプロピオン酸溶液0.24gと、80%のヒドラジン一水和物10gを150ミリリットルの純水に混合した液を添加し、1時間かけて酸化銅と反応させ、ゼラチンで被覆した銅微粒子を生成させた。その後、濾液比導電率が100μS/cm以下になるまで濾過洗浄し、窒素ガスの雰囲気で60℃の温度で10時間かけて乾燥し、ゼラチンで被覆した金属銅粒子を得た。
上記方法にて合成したゼラチンで被覆した平均粒子径50nmの金属銅粒子20gと高分子分散剤を溶解した有機溶媒(用いた高分子分散剤の種類、その酸価、アミン価、(アミン価−酸価)、添加量と有機溶媒の種類を表1に示す。)20gを混合・懸濁し、ペイントシェーカーにて1時間分散させ、金属銅分散液(試料A、B)を得た。
なお、ゼラチン、高分子分散剤の酸価、アミン価は前記のJIS K 7700あるいはASTM D2074に準拠した方法で測定した。
前記の金属銅分散液(試料A、B)をポリイミドフィルム(東レデュポン株式会社製 カプトン(登録商標)フィルム 300Vタイプ 75μm厚)にバーコーター#3で塗布し、金属銅含有膜を作製した。その後、(株)ニッシン製 MicroLabo-PSを用いて、プラズマ処理を次のように行い、金属銅焼結膜を得た。
まず、金属銅含有膜をプラズマ装置内の100℃又は150℃の所定温度に加熱したステージに置き、180秒又は30秒の所定時間加熱した。その後、装置内を60秒減圧し、3%H2−Heガスを装置内に30秒充填し、プラズマ照射を表2に記載の所定時間行った。プラズマ処理後、90秒、N2ガスをパージすることで冷却し、金属銅焼結膜を得た。
前記の試料Aを100ppm−O2−N2混合ガス気流中、200℃で予備加熱を行い、3%水素含有窒素ガス気流中250℃で行った。加熱には光洋サーモシステム社 電気管状炉(KTF085N)を使用し、昇温および降温は10℃/分とし、加熱時間は各工程とも1時間とした。
得られた金属銅焼結膜の表面と断面に白金を蒸着した後、走査型電子顕微鏡を用いて観察し、膜厚を測定した。また、金属銅焼結膜の体積抵抗値の測定には、ロレスタ−GP型低抵抗率計(三菱化学社製)を用いた。結果を表2、3に示す。本金属銅含有膜をプラズマ処理することで、加熱焼成法と同等に抵抗値の低い良好な金属銅焼結膜が得られた。
Claims (9)
- 少なくとも、ゼラチンを粒子表面に有する金属銅粒子、高分子分散剤及び有機溶媒を含む分散液を用いて基材の表面に金属銅含有膜を形成する工程(a)、
次いで、その金属銅含有膜の全領域又は一部領域にプラズマ処理する工程(b)を含む金属銅焼結膜の製造方法。 - 前記のゼラチンは、アミン価と酸価の差(アミン価−酸価)が0以下である、請求項1に記載の金属銅焼結膜の製造方法。
- 前記の高分子分散剤は、アミン価と酸価の差(アミン価−酸価)が0〜50である、請求項1又は2に記載の金属銅焼結膜の製造方法。
- 有機溶媒が、炭化水素、アルコール、ケトン、エステル、エーテル、グリコール、グリコールエーテル、グリコールエステルから選ばれる少なくとも1種である請求項1〜3のいずれか一項に記載の金属銅焼結膜の製造方法。
- メジアン径が1〜200nmである金属銅粒子を用いる請求項1〜4のいずれか一項に記載の金属銅焼結膜の製造方法。
- 製造された金属銅焼結膜の体積抵抗値が20μΩ・cm以下である、請求項1〜5のいずれか一項に記載の金属銅焼結膜の製造方法。
- 請求項1〜6のいずれか一項に記載の方法で製造された金属銅焼結膜を用いる電極。
- 請求項1〜6のいずれか一項に記載の方法で製造された金属銅焼結膜を用いる配線パターン。
- 請求項1〜6のいずれか一項に記載の方法で製造された金属銅焼結膜を用いる塗膜。
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